Solvothermal Synthesis and Characterization of Zn(NH 3 )CO 3 Single Crystal
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Solvothermal Synthesis and Characterization of Zn(NH3)CO3 Single Crystal Fushan Wen1,2,3, Jiesheng Chen2, Jin Hyeok Kim1*, Taeun Kim1 and Wenlian Li3 1
Photonic and Electronic Thin Film Laboratory, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-Dong Puk-Gu Kwangju South Korea, 500-757 2 State Key Laboratory of Inorganic Synthesis & Preparative Chemistry, College of Chemistry, Jilin University, 119 Jiefang Road，Changchun, 130023, P. R. China 3 Key Laboratory of the Excited States Process, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, Changchun, 130033, People’s Republic of China ABSTRACT A new 3-dimensional zinc carbonate Zn(NH3)CO3 has been synthesized from a glycol system with urea and zinc acetate as raw materials. The crystal structure and photoluminescent properties have been investigated using X-ray diffraction, smart CCD and FL. The compound had an orthorhombic system with space group of Pna21 with M = 142.41, a = 9.1449(18) Å, b = 7.5963(15) Å, c = 5.4982(11) Å, V = 381.95(13) Å3, Z = 4, R = 0.0285 and RW = 0.0745. The NH3 and CO32- were connected through the Zn-N bond and Zn-O bond in the symmetric unit. Photoluminescent property was observed in the compound at room temperature and the exited and emission peaks were located at about 350 nm and 426 nm, respectively.
INTRODUCTION Considerable interest has been focused on the study of luminescent properties of zinc compounds, such as ZnO [1], Zn2SiO4 [2] and other zinc complexes [3,4] because they can be used as photo- and electro- luminescent materials. Most of them were prepared by the traditional high temperature solid-state method. They have disadvantages of high temperature reaction process. There have been a few reports on the synthesis of those compounds by hydrothermal or solvothermal method which have been well known for their ability to get meta-stable compounds and to promote crystal growth [5]. Initially, we just tried to obtain nano-scale ZnO using solvothermal method in this study, but we obtained the Zn(NH3)CO3 single crystal instead of nano-ZnO. To our knowledge, Zn(NH3)CO3 has not been found in other reports. Therefore, we report the formation of the Zn(NH3)CO3 single crystal through the solvothermal method at relatively low temperature using the simple inorganic material, urea and simple organic solvent. Photoluminescent property of the title compound at room temperature will be discussed. EXPERIMENTAL To obtain the title compound, zinc acetate (Zn(CH3COO)2⋅2H2O) and urea (NH2CONH2) were used as the raw materials and the glycol (HOCH2CH2OH) was used as the organic solvent. In a typical synthesis procedure, an initial mixture with a molar composition of
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1Zn(CH3COO)2·2H2O: 4.4 (NH2)2CO: 53.7 EG was stirred for 12 hours, then sealed in a teflon-lined stainless steel autoclave and heated at 433 K for 108 hours. The reaction product was washed thoroughly with distilled water and dried at room temperature. The powder X-ray diffraction (XRD) da
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